• Title/Summary/Keyword: $^1H$-Nuclear Magnetic Resonance

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Synthesis and Characteristics of Partially Fluorinated Poly(vinylidene fluroide)(PVDF) Cation Exchange Membrane via Direct Sulfonation (직접술폰화반응에 의한 부분불소화 Poly(vinylidene fluroide)(PVDF) 양이온교환막의 합성 및 특성)

  • Kang, Ki Won;Hwang, Taek Sung
    • Membrane Journal
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    • v.25 no.5
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    • pp.406-414
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    • 2015
  • In this study, partially fluorinated cation exchange membranes were prepared by direct sulfonation of Poly(VDF-co-hexafluoropropylene) copolymers (PVDF-co-HFP) followed by a casting method for application in the Membrane capacitive deionization (MCDI). The structure of sulfonated PVDF-co-HFP (SPVDF) was confirmed by Fourier-transform infrared (FT-IR) and $^1H$ Nuclear magnetic resonance ($^1H$ NMR) analysis. For quantitative analysis of the chemical composition, the X-ray Photoelectron Spectroscopy (XPS) was used. The membrane properties such as water uptake, ion exchange capacity and electrical resistance were measured. It was suggested that the optimum direct sulfonation condition of PVDF-co-HFP ion exchange membranes was $60^{\circ}C$ and 7 hours for temperature and duration of sulfonation, respectively. The water uptake of the SPVDF ion exchange membrane was 21.5%. The ion exchange capacity and electrical resistance were 0.89 meq/g and $3.70{\Omega}{\cdot}cm^2$, respectively. It was investigated that if it is feasible to apply these membranes in MCDI at various cell potentials (0.9~1.5 V) and initial flow rates (10~40 mL/min). In the MCDI process, the maximum salt removal rate was 62.5% in repeated absorption-desorption cycles.

Synthesis and Characterization of a $Di-{\mu}-oxo-bridged$ Molybdeum(V) Complexes (두 개 산소 가교형 몰리브덴(V)착물의 합성과 그 성질에 관한 연구)

  • Kim, Il-Chool;Kim, Yeoung-Chan
    • Journal of the Korean Applied Science and Technology
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    • v.16 no.3
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    • pp.205-210
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    • 1999
  • The Mo(V) $di-{\mu}-oxo$ type $[Mo_2O_4(H_2O)_2L]Cl_2$ complexes(L: 4,4'-Diphenyl-2,2'-dipyridyl, 4,4'-Dimethyl-2,2'-dipyridyl, 4,7-Diphenyl-1,10-phenanthroline) have been prepared by the reaction of $[Mo_2O_4(H_2O)_6]^{2+}$ with a series of chelate ligands. These complexes are completed by two terminal oxygens arranged trans to one another and each ligand forms a chelate types. In $Mo_2O_4(H_2O)_2L$ two $H_2O$ coordinated at trans site of terminal oxgens. The prepared complexes have been characterized by elemental analysis, infrared spectra, electronic spectra, $^1H$ nuclear magnetic resonance spectra, and thermal analysis(TG-DTA). In the potential range -0.00V to -1.00V at scan rate of $50mVs^{-1}$, a cathodic peak at -0.83V ${\sim}$ -0.88V (vs SCE) and an anodic peak at -0.54V ${\sim}$ -0.88V (vs SCE) have been observed in aquous solution. The ratio of the cathodic to anodic current(Ipc/Ipa) is almost 2, we infer that redox is irreversible as dimer forms broken.

α-Glucosidase Inhibitor Isolated from Coffee

  • Kim, Shin-Duk
    • Journal of Microbiology and Biotechnology
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    • v.25 no.2
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    • pp.174-177
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    • 2015
  • A potent α-glucosidase inhibitor (compound I) was isolated from coffee brews by activity-based fractionation and identified as a β-carboline alkaloid norharman (9H-pyrido[3.4-b]indole) on the basis of mass spectroscopy and nuclear magnetic resonance spectra (1H NMR, 13C NMR, and COSY). The norharman showed potent inhibition against α-glucosidase enzyme in a concentration-dependent manner, with an IC50 value of 0.27 mM for maltase and 0.41 mM for sucrase. A Lineweaver-Burk plot revealed that norharman inhibited α-glucosidase enzyme uncompetitively, with a Ki value of 0.13 mM.

Gamakamide-E, a Strongly Bitter Tasting Cyclic Peptide with a Hydantoin Structure from Cultured Oysters Crassostrea gigas

  • Lee, Jong-Soo;Satake, Masayuki;Horigome, Yoichi;Oshima, Yasukatsu;Yasumoto, Takeshi
    • Fisheries and Aquatic Sciences
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    • v.15 no.1
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    • pp.15-19
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    • 2012
  • A new cyclic peptide (six-membered amino acid), gamakamide-E (L-Leu-L-Met (SO)-L-Me-Phe-L-Leu-D-Lys-L-Phe), was isolated as a strongly bitter tasting compound from cultured oysters, Crassostrea gigas. The molecular formula of $C_{43}H_{61}N_7O_8S$ was deduced from high resolution fast atom bombardment mass spectrometry (HR FAB-MS) ($[M+H]^+$ m/z 836.4356 ${\Delta}$= -2.4 mmu). Its unique structure including a hydantoin structure was firstly elucidated by nuclear magnetic resonance (NMR) analysis. Stereochemistries of constituent amino acids were determined by chiral high performanced liquid chromatography analysis of natural and synthesized peptides.

Solid-state NMR Studies of Phenethyl Sulfonic Acid-functionalized MCM-41

  • Chul Kim
    • Journal of the Korean Chemical Society
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    • v.68 no.2
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    • pp.74-81
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    • 2024
  • A sulfonic acid-water-silanol system in SO3H-functionalized MCM-41 was investigated using solid-state nuclear magnetic resonance techniques. The proton exchange rate between a water molecule and a silanol group in the S-PE-MCM-41 was determined by analyzing the 1D proton spectra, the proton EXSY spectrum, and 2H spin-lattice relaxation data under various hydration levels. Two kinds of water-bounding sites were found in the S-PE-MCM-41: weakly and strongly bound sites. Over several hours, water molecules bound to the weakly bound sites at the low hydration level migrated to the strongly bound sites. At high temperature, the S-PE-MCM-41 easily lost water molecules weakly bound to the silanol, while the strongly bound water molecules survived. Water molecules that participated in the hydration of the phenethyl sulfonate were involved in the hydrogenbonded silanol mechanism of proton conductivity. This phenomenon contributes higher proton conductivity to the S-PE-MCM-41 by the cooperation of sulfonyl and silanol groups in the proton transfer process, even at higher temperature.

Green flow injection spectrophotometric system for lead ion (II) evaluation in vegetables samples using new azo reagent

  • Fatimah Lateef Al-Zubaidi;Khdeeja Jabbar Ali
    • Analytical Science and Technology
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    • v.36 no.1
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    • pp.1-11
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    • 2023
  • A new, sensitive, and reliable flow injection methodology was investigated for the determination of lead ion (II) in vegetables' samples using a laboratory-prepared reagent 2-[(6-methoxy-2-benzothiazoly)azo]-4-methoxy phenol (6-MBTAMP). Infrared spectroscopy, UV-visible spectrophotometry, Energy dispersive X-ray spectroscopy (EDX), Elemental Analysis (CHN), nuclear magnetic resonance spectroscopy 1HNMR, and 13CNMR techniques were used to characterize the reagent and lead (II) complex. The method is based on lead ion (II) reacting with the reagent (6-MBTAMP) in a neutral solution to produce a green-red complex with a maximum absorbance at 670 nm. The optimum conditions, such as flow rate, lead ion (II) volume, reagent volume, medium pH, reagent concentration, and reaction coil length were thoroughly examined. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.621 mg·L-1 and 2.069 mg·L-1 , respectively, while Sandell's sensitivity was determined to be 0.345 ㎍·cm-2.

Alkyl Glycosides from the Flowers of Magnolia obovata (황목련 꽃으로부터 Alkyl Glycoside의 분리 동정)

  • Oh, Eun-Ji;Seo, Kyeong-Hwa;Kwon, Jung-Hwa;Lee, Dae-Young;Baek, Nam-In
    • Journal of Applied Biological Chemistry
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    • v.58 no.3
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    • pp.233-236
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    • 2015
  • The flowers of Magnolia obovata were extracted with aqueous MeOH and fractionated into EtOAc, n-BuOH, and $H_2O$ fractination. Three alkyl glycosides were isolated from the EtOAc fraction through repeated silica gel and ODS column chromatography. The structures were identified to be 2-methylbutan-1-ol-${\beta}$-$\small{D}$-galacto-pyranoside (1), 2-methylbutan-1-ol-${\beta}$-$\small{D}$-glucopyranoside (2), and 2-methylpropan-1-ol-${\beta}$-$\small{D}$-glucopyranoside (3) on the basis of spectroscopic analyses such as fast atom bombardment mass spectrometry, infrared spectroscopy, 1D nuclear magnetic resonance (NMR) ($^1H$ and $^{13}C-NMR$), and 2D NMR (gCOSY, gHSQC, and gHMBC). These compounds were isolated for the first time from the flower of M. obovata in this study.

Temperature and Pressure Dependence of the Nuclear Magnetic Relaxation Rates of -$NH_2$ Group in Thioacetamide / Acetone Solutions (티오아세트아미드 / 아세톤 용액의 아민기의 핵자기이완속도의 온도 및 압력 의존)

  • Kim Keon;Choi Young Sang;Yoon Chang Ju;E. Lang
    • Journal of the Korean Chemical Society
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    • v.36 no.1
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    • pp.33-37
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    • 1992
  • Information about $^{14}N$ relaxation rates is obtained for thioacetamide (TA) in acetone from a detailed line-shape analysis of the $^1H$ resonance signal of $NH_2$ group. The effect of pressure and of temperature were investigated, and activation energies for molecular reorientation are given. And also $^1H$ relaxation rates of $NH_2$ group of TA as a function of pressure and temperature are obtained. These results are discussed with the results for the $^{14}N$ relaxation of amine group.

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Flavonoid Glycosides from the Flowers of Pulsatilla koreana Nakai

  • Seo, Kyeong-Hwa;Jung, Jae-Woo;Nhan, Nguyen Thi;Lee, Youn-Hyung;Baek, Nam-In
    • Natural Product Sciences
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    • v.22 no.1
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    • pp.41-45
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    • 2016
  • Extraction and fractionation of Pulsatilla koreana flowers followed by, repeated open column chromatography for EtOAc and n-BuOH fractions yielded four flavonoid glycosides, namely, astragalin (1), tiliroside (2), buddlenoide A (3), and apigenin-7-O-(3"-E-p-coumaroyl)-glucopyranoside (4). The chemical structures of these flavonoid glycosides were elucidated on the basis of various spectroscopic methods including electronic ionization mass spectrometry (EI-MS), 1D NMR ($^1H$, $^{13}C$, DEPT), 2D NMR (gCOSY, gHSQC, gHMBC), and infrared (IR) spectrometry. This study represents the first report of the isolation of the flavonoid glycosides from the flowers of P. koreana.

Synthesis of Terpolymers and Dependence of Their Characteristics on Types and Content of High α-olefin

  • Kim, Jung Soo;Kim, Dong Hyun
    • Elastomers and Composites
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    • v.55 no.4
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    • pp.263-269
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    • 2020
  • Novel flexible terpolymers with a reactive moiety were synthesized by coordination polymerization with a metallocene catalyst and a cocatalyst system. C2-symmetric rac-Et(Ind)2ZrCl2 and tri-iso-butylaluminum/dimethylanilinium tetrakis (pentafluorophenyl) borate were employed as the catalyst and cocatalyst, respectively. We synthesized reactive terpolymers consisting of ethylene, a high α-olefin content (1-hexene, 1-octene, 1-decene, and 1-dodecene), and divinylbenzene. The structure and composition of the terpolymers were characterized by 1H-nuclear magnetic resonance analysis. The catalytic activity, polymer yield, molecular weight, and molecular weight distribution were measured as functions of the chain length and high content of α-olefins. Furthermore, the thermal properties and crystallinity of the terpolymers were determined by differential scanning calorimetry and wide-angle X-ray scattering.